DECCAN EDUCATION SOCIETY'S

FERGUSSON COLLEGE (AUTONOMOUS), PUNE

DEPARTMENT OF CHEMISTRY

F.Y. B. Sc Practicals -SEMESTER-II

LAB MANUAL 2020-21

S. No Title of the experiment

1 Determination of molar gas constants (R) in different units by
eudiometric method.
2 Preparation standard solution of 0.05N oxalic acid and
standardization and determination of strength of given 0.05N
(appro) KMnO4 solution.
3 Heat of solution of potassium nitrate in water.
4 Preparation of standard solution of oxalic acid and estimation of Fe
(II) by using standardized KMnO4 solution.
5 Polar plots of s, p and orbitals
6 Estimation of hydroxide/sulphate and carbonate present together
in mixture.
7 Relative viscosity of given organic liquids by viscometer
8 Determination of acetic acid in vinegar by titrimetric method.
9 Determination of rate constant of acid catalyzed ester hydrolysis.
10 Determination of percentage composition of ZnO and ZnCO3 in the
given mixture gravimetrically.
11 Acid-base titration using pH meter and Scientific graphing

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 1

EXPERIMENT 1: Determination of molar gas constants (R) in different units
by eudiometric method.

Aim: To determine the Molar Gas Constant (R) by eudiometric method and to express R in
different units.

Theory: The gas is the state of matter that is characterized by having neither a fixed shape
nor a fixed volume. Gases exert pressure, are compressible, have low densities and diffuse
rapidly when mixed with other gases. On the microscopic level, molecules or atoms in a gas
are separated by large distance and are constant motion. Four measurable properties are
used to describe a gas quantitatively; pressure (P), volume (V), and temperature (T) and
mole quantity (n). The relationship among these properties are studied by the gas laws viz;
Charles’s law, Boyle’s law, combined law etc.

The deal gas law is obtained by combination of Boyle’s law, Charles law, Avogadro’s
law, together

PV = nRT

P=Pressure of the gas (atmosphere), V=Volume of the gas (litres): n is the number of
moles of the gas in the sample; T is the gas temperature (Kelvin). R is the proportionality
constant called gas constant, and has theoretical value of 0.08206 l.atm.K-1mol-1 (8.314
J.mol-1.K-1). Different methods are used to determine gas constant includes, hydrogen
displacement method, oxide method, chloride method etc, Hydrogen displacement method
is convenient for metal those are more reactive than hydrogen. These metal displace
hydrogen from dilute solution of strong acid.

The volume of displaced hydrogen can be conveniently measured using a

eudiometer. Eudiometer is a long, volume measuring graduated glass tube closed at end.
The graduation enables us to measure the volume of the displaced hydrogen gas.

The pressure of liberated dry hydrogen gas will be calculated by using Dalton’s law of
partial pressure and temperature under which the hydrogen gas is collected will be
measured by thermometer. From the known quantity of magnesium and the stoichiometry
of the reaction, the number moles of hydrogen gas can be calculated.

Value of the gas constant R in different units :

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 2

 1) Value of R in C.G.S. unit :
Since 1 gram mole of any gas occupies a volume of 22.4 litres at S.T.P. condition, the
value of R can be calculated as follow :

P= 1 atmosphere = 76 cm of mercury

V= 22.4 litres = 22400 cm3

And T= 273 K

In C.G.S. system pressure 76 cm of mercury column

= 76 cm x density of Hg x gravitational acceleration

= 76 cm x 13.595 g cm-3 x 980.66 cm sec-2

=1013961.6 g cm-1 sec-2

= 1013961.6 ergs cm-3

PV 1013961.6 x 22400
R  for one gram mole of a gas
T 273

= 8.314 x 107 erg degree-1 mole-1

= 8.34 joule degree-1 mole-1 (1 joule=107 ergs)

2. Value of R in calories :

Since 1 calories = 4.18 x 10 7 ergs

And R = 8.314 x 107 erg degree-1 mole-1

 R = 8.32 x 107/4.18 x 107 =1.987 erg degree-1 mole-1

3. Value of R in litre atmosphere:

Since P = 1 atmosphere, V= 22.4 litres, T=273 K

PV 1x 22.4
R 
T 273

R= 0.08206 litre atmosphere degree-1 mole-1

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 3

Apparatus: Eudiometer, porcelain di plastic trough sh, scale, a large glass cylinder, beaker.

Chemicals: Metal piece (Mg), conc. Con. Hydrochloric acid, distilled water.

Diagram :

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 4

Procedure:

1. Clean the metal piece with sand paper. Weigh it accurately on a chemical balance
(Wg). [Note: Wt. of Mg ribbon should be between 32 to 40 mg]
2. Take 10-15 cm3 of conc. hydrochloric acid in the eudiometer and add 20-30 ml
distilled water. Stir the solution well and fill the eudiometer completely with
distilled water.
3. Take some water in plastic trough, putting the thumb on the eudiometer, invert it in
the trough, remove the thumb carefully .Take the precaution that, no air bubble
should enter the eudiometer.
4. Clamp the eudiometer in vertical position carefully.
5. Roll the metal piece and make it of a size which can be conveniently inserted in the
eudiometer.
6. Insert the piece in the eudiometer taking precaution that no air bubble should not
enter the eudiometer.
7. Metal react with acid, liberating hydrogen. The liberated hydrogen displaces the acid
from eudiometer. When the reaction is complete, the level of acid in the
eudiometer remains stationary. Wait for some time till the temperature of the acid
and hydrogen gas in the eudiometer becomes equal to room temaparture.
8. Measure the height of column of the solution (h cm) above the water level in trough.
Alternatively, adjust the height of column to ‘zero’ by leveling of endiometer in a big
jar filed with water. Also measure the volume of hydrogen gas (V) in the eudiometer.
Knowing the barometric pressure (B.P) of dry hydrogen gas (P) is calculate as
h
P  B.P.  [ PH 2O  ] (13.6 g cm-3 is the density of mercury)
13.6

PH2O is the aqueous tension at 0C

Insert your observation n in the observation table as shown below.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 5

 Reactions:

Mg + 2HCl → MgCl2 + H2 ↑

Observation Table:

Value
Trial-
No. Description of Observations Symbol and
I
Units

1. Wt. of metal piece W g

2. Volume of hydrogen gas liberated V cm3

3. Height of the solution in Eudiometer h cm

4. Room temperature in 0C t 0
C

Room temperature in 0K T = 273+ t K

5. Barometric Pressure B. P. cm

6. Aqueous tension at PH2O cm

Calculations:

1. Determination of pressure of dry H 2 at NTP [P] :

h
P  B.P.  [ PH 2O  ] = ------ cm (ρHg = 13.6 g.cm-3)
13.6

2. Determine mass of hydrogen gas (m) :

From the reaction,

Mg + 2HCl → MgCl2 + H2 ↑

We have 1 mole of Mg = 1 mole of Hydrogen

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 6

 24.312 g of Mg = 2 g of Hydrogen

W g of Mg = m g of Hydrogen

2W
m = -----g
24.312

Mass of liberate hydrogen gas =m= g

3. Determination of Molar gas constant[R] in different units.

1. R in lit.atm K-1 mol-1
According to the ideal gas equation, we have PV = nRT (n=m/2)

PV 2 PV
R =
nT mT

Where, R= molar gas constant in lit.atm K-1 mol-1

P=Pressure of dry hydrogen gas in atm.

V=volume of liberated hydrogen gas

m= mass of hydrogen gas

T= Temperature in K

2. R in cc.atm K-1 mol-1

According to the ideal gas equation, we have

PV 2 PV
R =
nT mT

R= molar gas constant in cc.atm K-1 mol-1

P=Pressure of dry hydrogen gas in atm.

V=volume of liberated hydrogen gas

m= mass of hydrogen gas

T= Temperature in K

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 7

 3. R in erg. K-1 mol-1
To obtain R in ergs the pressure of dry hydrogen gas must be expressed in
dynes per square centimeter and volume in cubic centimeter. The pressure of dry hydrogen
gas in dynes per centimeter square is given by the relation.

P=[Pressure of dry hydrogen in cm]x[Density of Hg at 0 oC in g cm-3]

x[Acceleration gravity in cm sec-2]

P= Pressure of dry hydrogen in cm x 13.595x980.66

P=……………………………… dynes cm-2

According to the ideal gas equation

PV 2 PV
R =
nT mT

Where, R= molar gas constant in erg K-1 mol-1

P=Pressure of dry hydrogen gas in atm.

V=volume of liberated hydrogen gas

m= mass of hydrogen gas

T= Temperature in K

4. R in joule. K-1 mol-1

 1 x 107 ergs = 1 joule

5. R in Cal K-1 mol-1

 4.184 joules = 1 cal

D. Determination of % error in R :

% Error = [Calculate R- Actual R] x100 / Actual R

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 8

Result Table:

Unit of R Expected value of R Observed value of R % Error

1. cc.atm K-1mol-1 82.05

2. lit.atm K-1 mol-1. 0.08205

3. erg. K-1 mol-1 8.314 x 107

4. Joule. K-1 mol-1 8.314

5. Cal. K-1 mol-1 1.987

Pressure of Water Vapour (Aqueous tension)

(In cm of Mercury)

Temp 0C Pressure Temp 0C Pressure Temp 0C Pressure

0 0.458 21 1.862 31 3.357

5 0.654 22 1.979 32 3.353

10 0.621 23 2.102 33 3.759

14 1.192 24 2.232 34 3.975

15 1.278 25 2.369 35 4.202

16 1.362 26 2.513 36 4.440

17 1.452 27 2.665 37 4.690

18 1.546 28 2.825 38 4.951

19 1.646 29 2.994 39 5.226

20 1.751 30 3.171 40 5.513

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 9

EXPERIMENT 2: Preparation standard solution of 0.05N oxalic acid and
standardization and determination of strength of given 0.05N (appro) KMnO4
solution.

Aim: a) Preparation 0.05 N Oxalic acid

b) Standardization of approximate 0.05 N KMnO4.

Chemicals & apparatus: H2C2O4 crystals, approx. 0.05 N KMnO4 solution, 2 N H2SO4,
burettes

Theory: Potassium permanganate is a secondary standard substance i.e. it changes its

composition on exposure to atmosphere. It is necessary to standardise KMnO4 titrating
against standard oxalic acid solution (primary standard) i.e. to determine the normality of
KMnO4 at the time of experiment, because the normality of KMnO4 solution changes on
keeping.

Procedure:

Part A: Preparation of 0.05 N Oxalic acid solution (Equivalent Wt. 63):

1000 cm3 1 N H2C2O4.2H2O ≡ 63 g of H2C2O4.2H2O

1000 cm3 0.05 N of H2C2O4.2H2O ≡ 63/ 20 g of H2C2O4.2H2O

100 cm3 0.05 N of H2C2O4.2H2O ≡ 63/ (20 x10) = 0.315 g of H2C2O4.2H2O

1. Weigh accurately 0.315 g of A. R. grade H2C2O4 powder on watch glass by means of

electronics balance.
2. Transfer it to clean beaker of 100 cm 3 capacities, add small amount of distilled water
and stir continuously till powder is dissolved. Transfer the solution in 100 cm3
volumetric flask using funnel. Collect the washing of watch glass & beaker 4 to 5
times with small amount of water. Dilute up to the mark and shake well.
3. Use this 0.05 N Oxalic acid solution for standardization of KMnO4 solution.
Part B: Standardization of given KMnO4 solution:

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 10

 1. Wash burette-1 with water, rinse and fill it with 0.05 N Oxalic acid solution & take 10
cm3 in conical flask.
2. Add 1 test tube 2 N H2SO4 ,warm the solution on wire gauge to about 60-70 0C. Do
not boil the solution. Heating is done till fumes are seen at the neck of flask.
3. Fill the burette-2 with, approx. 0.05N KMnO4 solution & titrate above hot solution of
Oxalic acid till the color of the solution become permanent faint pink, KMnO4 act as a
self indicator. Note this burette reading as ‘X’ cm3. Do not add KMnO4 very fast
otherwise brown coloured precipitate appears.
4. Repeat the same procedure twice & record the constant burette reading as ‘X’ cm 3.
Hence calculate the exact normality of KMnO4 solution.
Observations:

Part B: Standardization of given KMnO4 solution:

Given: 0.05 N H2C2O4

To find out: Normality of KMnO4

Solution by Burette -1: Standard 0.05 N Oxalic acid solution

[+ 1 test tube dil. H2SO4 (table reagent)

+ Heat till fumes are seen at the neck of conical flask]

Solution by Burette -2: Approx. 0.05 N KMnO4 solution

Indicator: KMnO4 solution self indicator

End Point: Colourless to permanent faint pink colour

Equation: i) 2 KMnO4 + 3 H2SO4 → K2SO4 + 2 MnSO4 + 3 H2O + 5(O)

ii) 5 H2C2O4 + 5 (O) → 5 H2O + 5 CO2

___________________________________________________________________________

2 KMnO4 + 3H2SO4+ 5H2C2O4 → K2SO4 + 2 MnSO4 + 3 H2O + 5 CO2

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 11

Observation Table:

Pilot I II III C.B.R. / cm3

Readings
(cm3) (cm3) (cm3) (cm3) X/ cm3

Final

Initial

Difference

Calculations:

Part B: Standardization of given KMnO4 solution:

N1V1 ≡ N2V2

KMnO4 ≡ H2C2O4

N1 x X ≡ 0.05 x 10

Exact Normality of KMnO4 = N1= 0.05 x 10 / X = _________ N

Strength of KMnO4 solution= Equivalent weight xNormality

Result:

1. C.B.R. for 10 cm3 of 0.05 N H2C2O4 solution X ________cm3 of KMnO4

2. Exact normality of KMnO4 solution N1 ________N

3. Strength of KMnO4 solution ________g/ litre

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 12

EXPERIMENT 3: Heat of solution of potassium nitrate in water.

Aim: To determine the heat of solution of potassium nitrate (KNO3) in water.

Chemical & apparatus: potassium nitrate (KNO3), hard glass tubes, stirrer, burette,

Thermometer (1/10th 0C), rubber cork, beaker etc.

Theory: - When a solute is dissolved in a solvent heat is either liberated or absorbed. Thus,
when sodium hydroxide is dissolved in water the solution becomes hot due to the heat
liberated. Potassium nitrate or ammonium chloride dissolves with absorption of heat, the
solution becomes cold due to this. The amount of heat liberated depends on the nature and
quantity of the solute, solvent, and temperature at which the solution is formed.

When one mole of a solute is dissolved in a finite quantity of solvent at specified

temperature the amount of heat liberated or absorbed {enthalpy change} is called integral
heat of solution. The integral heat of solution depends on the concentration of the solution.
Thus when one mole of hydrogen chloride is dissolved in 50 moles of water at 25 0C, heat
liberated is 17.51 k.cal. Thus

HCl(g) + 50 H2O(l) → HCl (50H2O) ∆H0298k = - 17.51 k.cal

(Note : Heat liberated is denoted by - ve sign, heat absorbed will be denoted by + sign.)
Similarly, HCl(g) + 200 H2O(l) → HCl (200H2O) ∆H0298k = - 17.74 k.cal

Changing the quantity of solvent in which 1 mole of solute is dissolved changes integral heat
of solution. Due to dilution of solution heat is either liberate or absorbed
called as an integral heat of dilution. [- 17.74 k.cal – (- 17.51 k.cal)] = - 0.23 k.cal

Suppose that 1 mole of solute is dissolved in large quantity of solvent such that no
measurable heat changes are observed on further diluting the solution., Such solution is
called infinitely dilute solution. The heat change accompanying the formation of infinitely
dilute solution is called of heat of solution.

HCl(g) + Aq. → HCl(aq) = - 17.96 k.cal

The heat change for given solute at a given temperature is found to be related to its
solubility at that temperature. The solubility of the solute may be defined as the weight of
the solute per 100 g i.e.100 cm3 of water. Solubility depends of nature of solute &
temperature. The equation that relates solubility (S), heat of reaction (∆H) & temperature
(T0 k) is

∆ .
=
LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 13
Assuming ∆H to be independent of temperature the equation (1) may be integrate

ΔH = 2.303R T1.T2 log (S2/S1) / (T2-T1) Cal.mol-1

Y = mX +C where C = constant of integration

To calculate (∆H) using eq.2 ,solublities at different temperatures are determined. The graph
of log S vs (1/T) is plotted ,the graph is staright line. The slope of the line is

(-∆H/2.303 R). From the slope (∆H) is calculated.

Alternatively, if S1 and S2 are the solubilities at two temperatures T1K and T2 K ,then,

log (S2/S1) = (- ∆H / 2.303 R) (T2 – T1) / T1.T2 ……(3)

∆H = 2.303 R ( T1T2 / T2 - T1 ) log S2/S1

The graph of S vs T is plotted. Two well separated points are selected (T 1 S1) and (T2 S2)

Procedure :

1. Weigh accurately 8 g of potassium nitrate (solute) & transfer it to hard glass tube.

2. Add 5 cm3 of distilled water (solvent) by burette in hard glass tube.

3. Close the tube with rubber cork fitted with a stirrer and thermometer.

4. Arrange the water bath as shown in figure taking sufficient water to dip the height of
solution in 250 cm3 beaker.

5. Heat the beaker on wire gauze & stir the solution till potassium nitrate (solute)
dissolve completely.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 14

 6. When the dissolution is complete, stop heating, lift up the hard glass tube (remove
from water bath) & cool the solution. During cooling continuously stirred the
solution till the crystal of KNO3 begins to appear (turbidity) & record this
temperature as a crystallization temperature at the solubility of KNO3 is 80 g /50
cm3.

7. Add 1 cm3 water to the glass tube, using the burette. Continue heating till a clear
solution is obtained & repeat the same procedure as mentioned above to record the
crystallization temperature.

8. Repeat the same procedure four time as mentioned above to record the
crystallization temperature adding every time 1 cm3 of water.

9. Calculate the solubility (S) in g per 100 cm3 water using

S = 100 x Weight of the salt / Volume of the water

Observation Table :

Wt. of Volume Crystlisation temp.

Solubility
Obs. the of the
(S) g/100 log S 1/ T
No. solute water 3 0
cm in C in K
(g) (cm3)

1 8 5

2 8 6

3 8 7

4 8 8

5 8 9

6 8 10

Graph & calculations :

1. Calculate the ΔH using the formula as shown below.

ΔH = 2.303R T1.T2 log (S2/S1) / (T2-T1) Cal.mol-1

(R = 2.Cal/K/.mol )

2. Plot the graph log S against (1/T) in K from the slope of the graph. Calculate ΔH.

Slope = ( - ΔH/2.303R ) (The slope of the line is negative , this will make ΔH positive.)

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 15

Result :

Heat of solution ΔH in Cal.mol-1

Name of the solute
By Calculation By Graph

Potassium Nitrate

Precaution :

1. Student should understand to read thermometer properly.

2. Continuous & vigorous stirring is very important at the time of cooling.
3. Use lens to read the thermometer (least count 0.1 0C).
4. Select proper scale to plot the graph.
5. Check the level of thermometer properly in hard glass tube (should not touch to
bottom)
6. Fit the hard glass tube with paper packing at the collar of tube only.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 16

EXPERIMENT 4: Preparation of standard solution of oxalic acid and estimation of Fe (II) by
using standardized KMnO4 solution.

Aim: a) Preparation 0.05 N Oxalic acid

b) Standardization of approximate 0.05 N KMnO4.

c) To find out the amount of iron (Fe-II) from the given solution.

Chemicals & apparatus: H2C2O4 crystals, approx. 0.05 N KMnO4 solution, 2 N H2SO4, burette
& given unknown solution of Iron (II) in 100 cm 3 volumetric flask.

Theory: Potassium permanganate is a secondary standard substance i.e. it changes its

composition on exposure to atmosphere. It is necessary to standardise KMnO4 titrating
against standard oxalic acid solution (primary standard) i.e. to determine the normality of
KMnO4 at the time of experiment, because the normality of KMnO4 solution changes on
keeping.

Fe (II) in the form of solution is a reducing agent. It undergoes oxidation when

reacted with KMnO4 in acidic medium. The standardization of KMnO4 and estimation of iron,
both are redox reactions. In these titrations, KMnO4 act as an oxidizing agent in acidic
medium.

Procedure:

Part A: Preparation of 0.05 N Oxalic acid solution (Equivalent Wt. 63):

1000 cm3 1 N H2C2O4.2H2O ≡ 63 g of H2C2O4.2H2O

1000 cm3 0.05 N of H2C2O4.2H2O ≡ 63/ 20 g of H2C2O4.2H2O

100 cm3 0.05 N of H2C2O4.2H2O ≡ 63/ (20 x10) = 0.315 g of H2C2O4.2H2O

4. Weigh accurately 0.315 g of A. R. grade H2C2O4 powder on watch glass by means of

electronics balance.
5. Transfer it to clean beaker of 100 cm 3 capacities, add small amount of distilled water
and stir continuously till powder is dissolved. Transfer the solution in 100 cm3
volumetric flask using funnel. Collect the washing of watch glass & beaker 4 to 5
times with small amount of water. Dilute up to the mark and shake well.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 17

 6. Use this 0.05 N Oxalic acid solution for standardization of KMnO4 solution.
Part B: Standardization of given KMnO4 solution:

5. Wash burette-1 with water, rinse and fill it with 0.05 N Oxalic acid solution & take 10
cm3 in conical flask.
6. Add 1 test tube 2 N H2SO4 ,warm the solution on wire gauge to about 60-70 0C. Do
not boil the solution. Heating is done till fumes are seen at the neck of flask.
7. Fill the burette-2 with, approx. 0.05N KMnO4 solution & titrate above hot solution of
Oxalic acid till the color of the solution become permanent faint pink, KMnO4 act as a
self indicator. Note this burette reading as ‘X’ cm3. Do not add KMnO4 very fast
otherwise brown coloured precipitate appears.
8. Repeat the same procedure twice & record the constant burette reading as ‘X’ cm 3.
Hence calculate the exact normality of KMnO4 solution.
Part C: Determination of Iron (Fe–II) from the given solution:

1. Dilute the given solution of Fe-II using distilled water up to the mark in 100 cm3
volumetric flask. Shake well.
2. Rinse the burette-1 with diluted Fe-II solution & take 10 cm3 in conical flask.
3. Add one test tube 2 N H2SO4 table reagent & titrate against standardized KMnO4
solution till the colour of the solution becomes permanent faint pink. Note this
burette reading as ‘Y’ cm3.
4. Repeat the same procedure thrice & record the constant burette reading as ‘Y’ cm3.
Hence calculate the exact amount of Fe-II solution.
Observations:

Part B: Standardization of given KMnO4 solution:

Given: 0.05 N H2C2O4

To find out: Normality of KMnO4

Solution by Burette -1: Standard 0.05 N Oxalic acid solution

[+ 1 test tube dil. H2SO4 (table reagent)

+ Heat till fumes are seen at the neck of conical flask]

Solution by Burette -2: Approx. 0.05 N KMnO4 solution

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 18

 Indicator: KMnO4 solution self indicator

End Point: Colourless to permanent faint pink colour

Equation: i) 2 KMnO4 + 3 H2SO4 → K2SO4 + 2 MnSO4 + 3 H2O + 5(O)

ii) 5 H2C2O4 + 5 (O) → 5 H2O + 5 CO2

___________________________________________________________________________

2 KMnO4 + 3H2SO4+ 5H2C2O4 → K2SO4 + 2 MnSO4 + 3H2O + 5 CO2

Observation Table:

Pilot I II III C.B.R. / cm3

Readings
(cm3) (cm3) (cm3) (cm3) X/ cm3

Final

Initial

Difference

Calculations:

Part B: Standardization of given KMnO4 solution:

N1V1 ≡ N2V2

KMnO4 ≡ H2C2O4

N1 x X ≡ 0.05 x 10

Exact Normality of KMnO4 = N1= 0.05 x 10 / X = _________ N

Part C: Determination of amount of Fe (II):

Given: Exact Normality of KMnO4

To find out : Amount of Fe in the given solution

Solution by Burette -1 : 10 cm3 diluted given Fe-II sample solution

Solution by Burette -2 : Standardised 0.05 N KMnO4 solution

Indicator: KMnO4 solution self indicator

End Point: Colourless to permanent faint pink colour

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 19

Equation: i) 2 KMnO4 + 3 H2SO4 → K2SO4 + 2 MnSO4 + 3 H2O + 5(O)

ii) 5 (O) + 10 FeSO4 + 5 H2SO4 → 5 Fe2(SO4)3 + 5 H2O

__________________________________________________________________

2 KMnO4 + 8 H2SO4 + 10 FeSO4 → K2SO4 + 2 MnSO4 + 5 Fe2(SO4)3 + 8 H2O

Observation Table:

Pilot I II III C.B.R. / cm3

Readings
(cm3) (cm3) (cm3) (cm3) Y/ cm3

Final

Initial

Difference

Part C: Determination of Fe-II:

2 KMnO4 ≡ 5 (O) ≡ 10 Fe

5 x 2 x (8 parts by weight of an oxygen) ≡10 Fe

8 parts by weight of an oxygen ≡ 1 Fe

1000 cm3 1 N KMnO4 ≡ 55.845 g of Fe

‘Y’ cm3 N1 N KMnO4 ≡ N1 x Y x 55.845 / 1000 x 1 g of Fe

≡ ‘A’ g of Fe in 10 cm3 diluted sample.

≡ ‘A x 10’ g of Fe in 100 cm3 diluted sample.

Result:

1. C.B.R. for 10 cm3 of 0.05 N H2C2O4 solution X ________cm3 of KMnO4

2. Exact normality of KMnO4 solution N1 ________N

3. C.B.R. for 10 cm3 of diluted Fe-II solution Y ________cm3 of KMnO4

4. Total Iron (Fe-II) in the given sample (A x 10) B ________g of Fe-II.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 20

EXPERIMENT 5: Polar plots of s, p and dz2 orbitals

Aim: To sketch the polar plots of s and p orbital.

Theory:

Polar and Rectangular Co-ordinates:

We are familiar with the Cartesian or rectangular co-ordinates that are mostly used in
rectangular systems e.g. building blocks etc.

If we look micro universe such as atoms, molecules or into macro universe such as galaxies,
stars, planets, etc. Their shapes are spherical or circular ones. To study such systems, polar
coordinates viz. r, ɵ and ɸ prove to be convenient against the rectangular one viz. x, y and z.
Rectangular co-ordinates can be converted into polar ones and vice-a-versa with the help of
trigonometry. This can be illustrated with the help of fig.1

Figure 1: Spherical polar co-ordinates

Electrons in the atoms have dual nature. An electron behaves like a particle (i.e.having mass
and localized) and it can also behave like a wave (i.e. having energy and delocalised). This
dual nature was used by Erwin Schrödinger to express or describe the electron in an atom.
Schrödinger’s wave equation (for electron wave) introduced a wave function ψ.

Theoretical description of the hydrogen atom (one electron system):

Schrödinger equation: H = E

 h2    2       1  2  Ze 2
H  2  sin   r   sin   
8 m  r  r      sin   2  r

The angular dependence of orbitals:

The angular function for 1S and 2S orbitals independent of ɵ and ɸ. Total wave function can
be written as the product of radial function R and angular function Y. Thus,

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 21

Ψ = R.Y, where R is radial part of function and Y is angular function.

Sketching s and p orbital:

To understand the shape of orbitals, angular functions are to be plotted against the angle ɵ
or ɸ. We know that angle ɵ varies from ɵ to and ɸ from 0 to 2π. Substitution of certain
values of ɵ or/and ɸ in function Y gives the corresponding angular function values. These
can be plotted by using a polar graph. The nature of polar graph paper is depicted in fig.2

This two dimensional graph paper is used to represent the relationship between angle ɵ and
angular function Y Angle ɵ or ψ can be selected on the circular scale of the paper and the
radial part of the function is scaled at distance from the centre of the graph on the line
corresponding to ɵ value (angle value).

S-orbital: The angular function for s orbital is Y0,0 (θ, ɸ) = ...............(1)

√

This function is independent of θ and ɸ. We plot Y0,0 against ɸ (from ɸ=0 to 2 ) in xy

plane. We get a circle in xy plane. For this plane z=0 and θ= 900 = . This is a static two-
dimensional representation for the function Y0,0. When this circle is rotated by 1800 about z-
axis, a three-dimensional surface in the form of a sphere is generated. This sphere is a three-
dimensional representation for Y0,0 or 1s orbital.

p-orbital: The angular wave functions for p-orbitals are:

pz: Y1,0 (θ, ɸ) = 3/4 cos θ

px: Y1,1 (θ, ɸ) = 3/4 sin θ. cos ɸ

pY: Y1,-1 (θ, ɸ) = 3/4 sin θ. sin ɸ

Among these function, Y1,0 does not involve angle ɸ and is the simplest one.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 22

Hence it is considered for plotting. To plot this function, select certain values of angles θ
from 0 to and hence calculate Y1,0. Table 3.2 represents one such set of θ0 and Y1,0 or pz
orbital.

Procedure

While drawing a polar plot of Y1,m against θ value is selected on the polar graph paper,
wherein a circular scale varying from 0 to 3600 is given. The function value for an angle θ is
graphed at the point on a line joining the centre of the graph paper and the point that
express the angle value. To sketch s and p orbitals on polar graph paper, take the scale along
the circular gridlines between 0 to ± 1 i.e. major gridlines as 0, ± 0.1, ±0.2...... ±1.0

s-orbitals:

i. Use angular wave function of s-orbitalsY0,0 (θ, ɸ) =

√
ii. Since =3.142,
Y0,0 (θ, ɸ)=0.282
iii. Y0,0 (θ, ɸ) is dependent of θ values. So mark 0.282 along the gridlines for all θ
values (0 to 360). Connect all points. The Circular shape of the s-orbital will be
appeared which be spherical in 3-dimensions.

Table-1

 R =  R =  R =  R =
1/2 1/2 1/2 1/2
o o o o o
0 /360 0.282 90 0.282 180 0.282 270 0.282
o o o o
10 0.282 100 0.282 190 0.282 280 0.282
o o o o
20 0.282 110 0.282 200 0.282 290 0.282
o o o o
30 0.282 120 0.282 210 0.282 300 0.282
o o o o
40 0.282 130 0.282 220 0.282 310 0.282
o o o o
50 0.282 140 0.282 230 0.282 320 0.282
o o o o
60 0.282 150 0.282 240 0.282 330 0.282
o o o o
70 0.282 160 0.282 250 0.282 340 0.282
o o o o
80 0.282 170 0.282 260 0.282 350 0.282

p-orbitals:

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 23

 i. Use angular wave function of px orbital
Y1,0 (θ, ɸ) = 3/4 cos θ
ii. Substitute value of θ ranging from 0 to 3600 with difference of 100 and calculate
Y1,0(θ, ɸ) eg. θ = 1800.
Y1,0 (θ, ɸ) = 3/4 cos θ
= R (-1.00)
iii. Tabulate the data as per Table -2
iv. Plot Y1,0(θ, ɸ) values for respective angle along the gridlines as per scale.
v. Connect all points plotted. P-orbital (two lobes) will appear.
vi. Similarly pxand py orbital can be sketched. Their shapes will be same with same
the orientations along X and Z axes respectively.
See fig. Repeat this procedure again on other half of the graph paper for same θ
and function values.

Table 2. Values of Y1,0 (θ) for various angles θ

 R =  R =  R =  R =
(3/4)1/2 (3/4)1/2 (3/4)1/2 (3/4)1/2
o o o o o
0 /360 1.00 90 0.00 180 − 1.00 270 0.00
o o o o
10 0.98 100 − 0.17 190 − 0.98 280 0.17
o o o o
20 0.94 110 − 0.34 200 − 0.94 290 0.34
o o o o
30 0.87 120 − 0.50 210 − 0.87 300 0.50
o o o o
40 0.77 130 − 0.64 220 − 0.77 310 0.64
o o o o
50 0.64 140 − 0.77 230 − 0.64 320 0.77
o o o o
60 0.50 150 − 0.87 240 − 0.50 330 0.87
o o o o
70 0.34 160 − 0.94 250 − 0.34 340 0.94
o o o o
80 0.17 170 − 0.98 260 − 0.17 350 0.98

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 24

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 25
LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 26
Experiment 6: Estimation of hydroxide and carbonate present together in
mixture.
Aim: To determine the amount of sodium carbonate (Na2CO3 ) and sodium hydroxide
(NaOH) from a given mixture by titrating against a standard solution of 0.05 N HCl.

Theory: The experiment involves neutralization (acid-base) reaction. A double titration is

carried out in two stages with a suitable indicator at each stage. The method is called as two
indicator method.

Phenolphthalein is extremely sensitive towards hydrogen ions. It has a pH range of

about 8 to 10 and shows the colour change when sodium hydroxide (strong base) is
completely neutralized and sodium carbonate is converted to bicarbonate i.e. Na2CO3 is half
neutralized.

Thus, NaOH + HCl NaCl + H2O

Na2CO3 + HCl  NaHCO3 + NaCl

Methyl orange has pH range 3.2 to 4.4. Thus during the titration of alkali mixture
with HCl solution, using methyl orange indicator, more amount of HCl solution is required to
be added so that the pH of the solution becomes 3.2 to 4, when methyl orange changes the
colour of the solution. At this second stage, both NaOH and Na2CO3 are completely
neutralized. Na2CO3 reacts with HCL in both stages while NaHCO3 reacts only in second
stage.

Thus,

Na2CO3 + 2HCl  2NaCl + H2O + CO2

NaHCO3 + HCl  H2CO3 + NaCl

The method consists of titrating alkali mixture, with standard solution of HCl using
phenolphthalein for the first reading and then continuing the titration with the addition of
methyl orange to the same solution for the second reading. (Alternatively the titrations may
be performed separately by using these indicators.) From these readings the amount of HCl
solution required for neutralization of NaOH alone and that for neutralization of Na 2CO3
alone can be found out and hence the amount of NaOH and Na 2CO3 present in the given
solution can be calculated.

Chemicals :

i) HCl (0.05 N exact)

ii) Phenolphthalein indicator
iii) Methyl orange indicator
iv) Mixture of NaOH and Na2CO3 solution.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 27

Procedure :

1. Fill Burette-1 with 0.05 N HCl solution.

2. Dilute the given solution ( mixture of NaOH + Na2CO3) to 100 ml with distilled
water. Shake it well.
3. From Butette-2, take 10 ml of the diluted solution of mixed alkalis in a conical flask.
4. Add 2 to 3 drops of phenolphthalein indicator. The solution becomes pink.
5. Add drop by drop HCl solution from Burette-1 to this mixture till pink colour just
disappears. This is the end point of the first titration. Call this burette reading V 1 ml.
6. To this decolourised (i.e. colourless) solution, add 2 to 3 drops of methyl orange
indicator. The solution turns yellow.
7. Continue the addition of HCl from burette-1. Shake the flask after each addition.
8. At the end point, the colour of the solution changes from yellow to orange red. Call
this burette reading V2 ml.
9. Repeat the procedure and find out constant burette readings.

Observation Tables:

Burette 1: HCl Solution (0.05 N)

Burette 2: Diluted alkali mixture solution
Given : HCl solution (0.05 N)
Indicator: Phenolphthalein (1st step), Methyl orange (2nd step)
End Point: Pink to colourless and for second step, yellow to orange red

Equations:

Ist step

NaOH + HCl NaCl + H2O

Na2CO3 + HCl  2NaHCO3 + NaCl

B. R. Pilot/ ml I /ml II /ml III/ml C.B.R. /ml

Final
Initial V1 =
Diff.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 28

IInd step

Na2CO3 + 2HCl  2NaCl + H2O + CO2

NaHCO3 + HCl  H2CO3 + NaCl
B. R. Pilot/ ml I /ml II /ml III/ ml C.B.R./ ml
Final
Initial V2 =
Diff.

Calculations:

(1) To find out the amount of Na2CO3

Phenolphthalein reading = V1 ml = Volume of HCl required for complete neutralization of

NaOH and half of Na2CO3.

Methyl orange reading = V2 ml = Volume of HCl required for complete neutralization of

Na2CO3

(V2 – V1) ml = Volume of HCl required for half neutralization of Na2CO3.

 Volume of 0.05 N HCl required for complete neutralization of Na 2CO3 in 10 ml of diluted
solution = 2 (V2 – V1) ml
But, 1000 ml 1 N HCl = 53g Na2CO3
2(V2  V1 )  0.05  53
 2 (V2 – V1) ml 0.05 N HCl =  X g Na2CO3
1000

Since, 10 ml diluted solution contains = X g Na2CO3

100 ml diluted solution = 10 * X g Na2CO3.
2) To find out the amount of NaOH:
Volume of 0.05 N HCl required for neutralization of NaOH
= V2 – Volume of HCl required for neutralization of Na2CO3
= V2 – 2 (V2 – V1) ml
= 2V1 – V2 = . . . . . ml
But, 1000 ml 1 N HCl = 40g NaOH
(2V1  V2 )  0.05  40
(2V1 – V2) ml 0.05 N HCl =  Y g NaOH
1000

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 29

10 ml diluted solution = Y g NaOH

 100 ml diluted solution = 10 x Y g NaOH.

Result Table

1 Titration reading with phenolphthalein ………. ml

2 Titration reading with methyl orange ………. ml
3 Amount of Na2CO3 in the given solution ……….g
4 Amount of NaOH in the given solution ……….g
Note : By this method , commercial sample of caustic soda (NaOH) which contains small
quantities of Na2CO3 and H2O is analyzed.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 30

EXPERIMENT 7: Relative viscosity of given organic liquids by viscometer

Aim : Determination of the relative viscosity of given liquids at room temperature by

Ostwald viscometer.

Material : Ostwald viscometer, specific gravity bottle, stop watch, alcohol (washing solvent),
Liquid A, B, C and water.

Theory : Liquids exhibit resistance to flow known as viscosity . More precisely the resistance
experienced by one layer in moving past another layer is called the viscosity which
consequently can be regarded as a type of internal friction. Coefficient of viscosity denoted
by ‘η’ and is defined as force in dynes per unit area (sq. cm) required to cause two parallel
layer of liquid one centimeter apart, to slide past each other with a velocity of one
centimeter per second. Unit of viscosity under such conditions is poise.

The viscosity of a liquid is usually measured by observing the rate of flow of liquid
through some form of capillary tube. The flow of homogeneous liquid through a capillary
tube is governed by Poiseuille equation.

r 4t r 4t
V 
8l 8Vl

Where η = coefficient of viscosity

ρ = driving force (pressure difference between two layers)

r = radius of the capillary tube in cm

V = volume in cm3 of the liquid

Although the values of all the variables in this equation can be determine
experimentally & absolute viscosity can be calculated, the procedure is tedious one. So
usually viscosity determination is relative to a reference liquid of known value of η.

In the Ostwald viscometer for the two liquids time is noted when same volume
(contain between two fix marks) is allowed to flow through the same capillary tube.
Naturally for the two liquids (one of which is the reference liquid) v, l & r are constant. ‘p’ is
the driving force will be equal to hydrostatic pressure on the liquid.

P  h g

Where h = height through which liquid falls

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 31

 ρ = density of the liquid

g = acceleration due to gravity

Though this will vary during the course of experiment, for both the liquids initial &
final values of h will be same and so ‘p’ will be proportional only to their densities. Therefore
under condition of Ostwald viscometer the relative viscosities of two liquids will be directly
proportional to their densities and relative times taken by them for the flow of same
volume.

A A tA
Relative Viscosity of liquid =  .
W W tW

Diagram :

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 32

Procedure : Part-A : Viscosity (Flow time) measurement -

1. Wash & dry viscometer using alcohol & dries respectively.

2. Fix the clean & dry viscometer vertically.
3. Pour exactly 15 cm3 of pure liquid B (distilled water) from E end of viscometer.
4. Suck the liquid through the capillary end using rubber tube just above the mark U,
keep a stop watch ready.
5. Release the liquid to flow back. Start the stop watch when the meniscus passes the
upper mark U. Record the time required to flow the liquid from mark U to L as a flow
time in seconds.
6. Record flow time two more time for same solution in the same position to avoid
personal error & record the mean of flow time.
7. Repeat the same procedure for all the liquids A,B, C.
Part-B : To determine density of liquids (ρ) -

1. Wash & dry specific gravity bottle using alcohol & dries respectively.
2. Note a weight of empty specific gravity bottle with stopper on electronic balance.
Completely fill up the specific gravity bottle with liquid B (distilled water) & keep the
stopper. Note the weight of bottle with liquid.
3. Repeat the same procedure for all the liquids A,B, C.
4. Calculate the density (specific gravity) of all the liquids taking ratio of weight of
liquid to weight of the distilled water.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 33

Observations :

Weight of empty specific gravity bottle (y): ___________ g.

Observation Table :

=
Weight of liquid /weight of water
Weight of bottle + liquid (x) / g

(g.cm-3)
Flow time / sec

Weight of liquid (x-y) / g

ρ x t (g.cm-3.s)
1 2 3 Mean

Density
Liquid

Water (W)

Calculation :
A A tA
Relative Viscosity of liquid =  .
W W tW
e.g. ηA = viscosity of liquid A
ηW= viscosity of liquid water
ρA = density of liquid A
ρW = density of liquid water
Precautions :

1. Wash & dry viscometer whenever solution changes.

2. Detach the rubber tube at the time of washing & drying.(Rubber dissolve in washing
solvent)
3. Arrange viscometer vertically.
4. Volume of solution should be taken by burette or pipette only.
5. Wipe out specific gravity bottle by filter paper before weighing.
Result : 1. Relative viscosity of A = ____________

2. Relative viscosity of B = ___________

3. Relative viscosity of C = ____________

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 34

EXPERIMENT: 8 Determination of acetic acid in vinegar by titrimetric method.

Aim: a) Preparation of 0.05 N Oxalic acid.

b) Standardization of approximate 0.05 N NaOH
c) To find out the amount of acetic acid in vinegar.

Chemicals & apparatus: H2C2O4 crystals, approx. 0.05 N NaOH solution, Phenolphthalein,
burette & given unknown solution of Vinegar in 100 cm3 volumetric flask.

Theory: Sodium hydroxide is standardised by titrating it against standard oxalic acid solution
i.e. to determine the exact normality of NaOH at the time of experiment.

In commercial vinegar, 4-5% acetic acid is present. Acetic acid is a weak acid and can be
titrated against strong base like NaOH using phenolphthalein as an indicator and its
percentage can be found out.

Procedure:

Part A: Preparation of 0.05 N Oxalic acid solution (Equivalent Wt. 63):

1000 cm3 1 N H2C2O4.2H2O ≡ 63 g of H2C2O4.2H2O

1000 cm3 0.05 N of H2C2O4.2H2O ≡ 63/ 20 g of H2C2O4.2H2O

100 cm3 0.05 N of H2C2O4.2H2O ≡ 63/ (20 x10) = 0.315 g of H2C2O4.2H2O

1. Weigh accurately 0.315 g of A. R. grade H2C2O4 powder on watch glass by means of

electronics balance.

2. Transfer it to clean beaker of 100 cm 3 capacities, add small amount of distilled water
and stir continuously till powder is dissolved. Transfer the solution in 100 cm3
volumetric flask using funnel. Collect the washing of watch glass & beaker 4 to 5
times with small amount of water. Dilute up to the mark and shake well.

3. Use this 0.05 N Oxalic acid solution for standardization of NaOH solution.

Part B: Standardization of given NaOH solution:

1. Wash burette-1 with water, rinse and fill it with 0.05 N Oxalic acid solution & take 10
cm3 in conical flask.

2. Add two drops of phenolphthalein indicator.

3. Fill the burette-2 with, approx. 0.05NNaOH solution & titrate above solution of oxalic
acid till the color of the solution become permanent faint pink, Note this burette
reading as ‘X’ cm3.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 35

 4. Repeat the same procedure twice & record the constant burette reading as ‘X’ cm3.

5. Then calculate the exact normality of NaOH solution.

Part C: Determination of acetic acid in the given vinegar solution:

1. Dilute the given solution of vinegar using distilled water up to the mark in 100 cm3
volumetric flask. Shake well.

2. Rinse the burette-1 with diluted vinegar solution & take 10 cm3 in conical flask.

3. Add two drops of phenolphthalein & titrate against standardized NaOH solution till
the colour of the solution becomes permanent faint pink. Note this burette reading
as ‘Y’ cm3.

4. Repeat the same procedure thrice & record the constant burette reading as ‘Y’ cm 3.

5. Then calculate the exact amount of Acetic acid in the given vinegar solution.

Observations:

Part B: Standardization of given NaOH solution:

Given: 0.05 N H2C2O4

To find out: Normality of NaOH

Solution by Burette -1: Standard 0.05 N Oxalic acid solution

Solution by Burette -2: Approx. 0.05 N NaOH solution

Indicator: Phenolphthalein

End Point: Colourless to permanent faint pink colour

Observation Table:

Pilot I II III C.B.R. / cm3

Readings
(cm3) (cm3) (cm3) (cm3) X/ cm3

Final

Initial

Difference

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 36

Calculations:

Part B: Standardization of given NaOH solution:

N1V1 ≡ N2V2

NaOH ≡ H2C2O4

N1 x X ≡ 0.05 x 10

Exact Normality of NaOH = N1= 0.05 x 10 / X = _________ N

Part C: Determination of amount of Acetic acid:

Given: Exact Normality of NaOH

To find out: Amount of Acetic acid in the given vinegar solution

Solution by Burette -1: 10 cm3 diluted given vinegar solution

Solution by Burette -2: Standardised 0.05 N NaOH solution

Indicator: Phenolphthalein

End Point: Colourless to permanent faint pink colour

Observation Table:

Pilot I II III C.B.R. / cm3

Readings
(cm3) (cm3) (cm3) (cm3) Y/ cm3

Final

Initial

Difference

Part C: Determination of Acetic acid:

NaOH+ CH3COOH → CH3COONa + H2O

1 mole of NaOH= I mole of CH3COOH

1000ml 1N NaOH= 60.5 g of CH3COOH

‘Y’ cm3( N1) N NaOH ≡ N1 x Y x 60.05 / 1000 x 1 g = ‘A’ g of CH3COOH

10m 10ml of diluted vinegar=‘A’ g of CH3COOH

100ml of diluted vinegar=‘A’X10 g of CH3COOH = ‘B’ g of CH3COOH

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 37

W g of vinegar=‘B’ g of CH3COOH

100g of diluted vinegar=‘B’X100/W= Z % of CH3COOH

Result:

1. C.B.R. for 10 cm3 of 0.05 N H2C2O4 solution X ________cm3 of NaOH

2. Exact normality of NaOH solution N1 ________N

3. C.B.R. for 10 cm3 of diluted vinegar solution Y ________cm3 of NaOH

4. Total amount of acetic acid in the given B ________g

100vinegar sample (A x 10)=B

5. Percentage of acetic acid in Vinegar Z%

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 38

EXPERIMENT:9 Determination of rate constant of acid catalyzed ester hydrolysis

Aim:- To determine the rate constant of acid catalysed ester hydrolysis.

Apparatus :- Stopper bottle, conical flask, beaker, water bath, stop-watch,

burettes, etc.

Chemical:- Methyl acetate, 0.5N HCl, 0.1N NaOH, phenolphthalein, etc.

Theory:- The chemical reaction of methyl acetate in presence of hydrochloric acid is

represented as

dil HCl
CH3COOCH3 + H2O CH3COOH +CH3OH

In this reaction the concentration of water is in excess and practically

concentration of water remains constant. The rate reaction only depend on concentration
of methyl acetate only. This is example of pseudo unimolecular reaction. According to law of
mass action, the rate this reaction can be written as

− = [CH3COOH]

The proportionality constant is known as the rate constant of the first order reaction. For an
first order reaction, k should be constant and characteristic of the reaction. It is independent
on the concentration of the reactant. It depends on the temperature. The rate constant of
this reaction is given as

2.303
= log
( − )

k- Rate constant of the first order reaction

a- Initial concentration of the reactant

x- Concentration of the reactant reacted in time t

(a-x)- Concentration of reactant left at time t

Procedure:-

1. Take 100 ml 0.5 N HCl solution in clean stopper bottle . keep this bottle in water bath
to attain the constant temperature.

2. Fill the 50 ml burette with 0.1 N NaOH.

3. Take few pieces of ice and 2-3 drops of phenolphthalein indicator in a conical flask.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 39

 4. By common burette add exactly 5 ml methyl acetate in the stopper bottle of
hydrochloric acid, stir well and note the time of mixing(T0). Immediately pipette out
5ml of the reaction mixture in conical flask containing ice and indicator.

5. Immediately titrate this reaction mixture against 0.1 N NaOH till faint pink persisting
for a minute and note this burette reading as the T0.

6. After 10 minute pipette out 5 ml reaction mixture from stopper bottle in conical flask
containing ice and indicator.

7. Repeat the same procedure at regular time intervals of 10 minutes up to 50 minutes

from the T0 time.

8. Plot the graph log a/(a-x) against time (t), find the slop and calculate the rate
constant of the reaction.

Observation:-

Initial reading (T0) = ----------ml.

Infinite reading (T) = --------ml (Given).

Initial concentration a = (T- T0) = ---------ml.

Observation table:-

Sr. Time(t) Burette x= (a-x) = Log[a/(a-x)] k Mean k

No. ml Reading (Tt) (T-Tt) min-1
(Tt-T0) min-1
ml

10

20

30

40

50

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 40

Calculation:-

Calculate the rate constant by using Equation

. .
= log = log ∞
= -------- min-1
( ) ∞

Where

a =(T-T0) = initial concentration

t = time in minute

(a-x) = (T-Tt) = concentration at time t

Calculate the rate constant by Graphical Method

Plot the graph of Log[a/(a-x)] versus t. A linear plot passing through origin with
slope =k/2.303 will be obtained and k can be calculated by the

equation, k = slope x 2.303.

Slope =

Graph:-

Result:- The Rate constant k of first order acid catalysed hydrolysis of methyl acetate

1) By Calculation = ---------- min-1

2) By Graph = ----------- min-1

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 41

EXPERIMENT: 10 Determination of percentage composition of ZnO and ZnCO3 in the given
mixture gravimetrically.

Aim: To determine the % composition of ZnO and ZnCO3 from the given mixture
graivimetrically.

Chemicals & apparatus: Mixture of ZnO and ZnCO3, desiccator, crucible, pair of tongs, pipe
clay triangle, asbestos sheet, tripod stand & wire gauge.

Theory: Mixture of ZnO and ZnCO3 on heating loses CO2 from ZnCO3 but ZnO remains
unchanged in chemical composition. Thus there is loss in weight due to escape of CO2 from
ZnCO3. From this loss in weight, amount and percentage of ZnCO3 can be calculated.

Equation : ZnCO3 → slow hea ng→ ZnO + CO2 ↑

Procedure :

1. Heat the clean & dry crucible with lid on a blue flame for 5 minutes to remove the
moisture, on a pipe clay triangle using oxidizing flame.
2. Remove the flame & allow the crucible with lid to cool on an asbestos sheet. Keep it
in desiccator for drying.
3. Weigh the empty crucible on electronic balance & note the weight as W 1 g.
4. Take 0.5 to 0.6 g of given mixture in crucible by means of spatula & weigh accurately
the crucible, note the weight as W2 g.
5. Heat the crucible over medium and blue flame gently on a pipe clay triangle for 45
minutes.
6. Cool the crucible on an asbestos sheet & dry it in a desiccator & then weigh the
crucible with residue as W3 g.
7. Repeat the process of heating, cooling & weighing till a constant weight is obtained.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 42

Observation Table :

Sr. No. Description Symbol Weight

1. Weight of the empty crucible W1 g

2. Weight of the crucible + substance W2 g

3. Weight of the substance taken X = W 2 - W1 g

4. Weight of the crucible + residue W3 g

5. Loss in Weight Y = W 2 - W3 g

Calculation :

1. Calculation of amount of ZnCO3(A) :

I mole of CO2 ≡ 1 mole of ZnCO3

44g of CO2 ≡ 125.39g of ZnCO3

Y g loss in weight of substance ≡ ______A g of ZnCO3

A g of ZnCO3 ≡ Y x125.39/44

Weight of ZnCO3 ≡ _______ A g of ZnCO3

2. Calculation of amount of ZnO( B) :

Amount of ZnO ( B) = Weight of substance taken( X)- Weight of ZnCO3(A)

Amount of ZnO ( B) = (X-A) g

3. Calculation of % of ZnCO3 in mixture:

% of ZnCO3 in mixture(C) = Weight of ZnCO3(A) x100/ Weight of substance taken( X)

% of ZnCO3 in mixture(C) = Ax100/X

4 Calculation of % of ZnO in mixture(D):

% of ZnO in mixture(D) = 100-% of ZnCO 3 (C)

% of ZnO in mixture(D) = 100-C

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 43

Result :

Sr. No. Description Symbol Weight

1. Weight of the substance taken X = W 2 - W1 g

2. Loss in Weight Y = W 2 - W3 g

3. % of ZnCO3 in mixture C g

4. % of ZnO in mixture D g

Precaution:
 Avoid strong heating
 Always keep crucible on asbestos sheets only.
 Do not weigh crucible in hot condition
 Use always oxidizing flame for heating crucible.
 Carry crucible in desiccator only, which contains desiccants.
 Always operate the crucible using pair of tongs only.

LAB MANUAL- F.Y .B.Sc. CHEMISTRY, SEM II 2020-21 Page 44

FERGUSSON COLLEGE (AUTONOMOUS), PUNE
Department of Chemistry

ACID-BASE TITRATION USING A pH METER

INTRODUCTION

In an acid-base titration, the important information to obtain is the equivalence point. If

there are a given number of moles of acid in the titration flask, the equivalence point is reached
when that same number of moles of base has been added from the burette. The molarity of the
base can then be calculated since the number of moles of base added is the same as the number of
moles of acid in the flask, and the volume of the base added is also known. Similarly, if the
number of moles of acid in the titration flask is unknown, it can be calculated for the equivalence
point if the molarity of the base and the volume of base added are known. Often the pH of the
solution will change dramatically at the equivalence point.
In a pH-metry/potentiometric acid-base titration, an indicator is not necessary. A pH
meter is used to measure the pH as base is added in small increments (called aliquots) to an acid
solution. A graph is then made with pH along the vertical axis and volume of base added along
the horizontal axis. From this graph the equivalence point can be determined and the molarity of
the base calculated.
LEARNING OBJECTIVES
1. To perform a potentiometric titration of an acidic solution of known molarity.
2. To graph the volume of base added vs the pH and to determine the equivalence point.
3. To calculate the molarity of the monobasic acid solution.
MATERIALS
pH meter with standard buffers of pH 4.0, pH 7.0, and pH 9, micro burette, magnetic stirring bar,
100 ml beaker, acid solution unknown normality and NaOH Solution of known normality.
PROCEDURE
1. Obtain exactly 10 mL of 0.01 N monobasic acid in a clean beaker. Never pour any
solution back into this beaker.
2. Rinse your burette with distilled water. Then use a small amount of the 0.05 N NaOH
solution to rinse the burette. Pour the NaOH solution into the burette. Let some of it flow
through the tip. Pour the rest of the NaOH solution out the top of the burette, rotating the
burette as you pour. The rinsing solution should be discarded into the sink. Repeat this
rinsing procedure twice more. Fill the burette to some point higher than the markings
with the NaOH solution and then carefully let the NaOH solution out into a waste
container until the bottom of the meniscus is on the 0.00 line.
4. Standardize the pH meter-Set the temperature, dip the combined electrode in pH-7 buffer
solution, set pH-7 by calibration knob. Wash and clean the electrode. Dip the electrode in
pH-4 buffer solution and set the pH-4 by adjusting slope knob. (Back side of pH meter)
5. Place a 100 mL beaker under the burette containing the monobasic acid and let out
exactly 10 mL of acid into the beaker.
6. Carefully drop a magnetic stirring bar into the beaker containing the monobasic acid
solution. Set the beaker on the magnetic stirring motor and position the burette
containing the NaOH solution and the pH electrode. Carefully turn on the stirring motor
and make sure that the stirring bar does not hit the electrode.
7. Set up your data table to include mL of NaOH added and the pH of the solution. You

1
FERGUSSON COLLEGE (AUTONOMOUS), PUNE
Department of Chemistry

should allow for as many as 4 mL of solution.

8. Measure and record the pH of the solution before any NaOH has been added.
9. Add 0.2 mL of NaOH solution carefully from the burette. Record the pH when it has
stabilized. Add another 0.2 mL of NaOH and record the pH. Continue adding NaOH in
0.2 mL increments until you have obtained a pH reading greater than 12 pH.
10. Remove the electrode from the solution, rinse it with distilled water, and store it as
directed by your teacher.
11. The solutions may be discarded down the sink. Rinse the burette with distilled water
and place it upside down in the burette holder to drain.
OBSERVATION TABLE:
Mean of ml of
pH/V
SN ml of NaOH Added pH NaOH added

1 0.0
2 0.2
…..
20 4.0

CALCULATIONS
1. Make a graph of the pH vs mL of NaOH added. The pH should be on the vertical axis
and the mL of NaOH should be on the horizontal axis the pH scale is spread out as
much as possible.
2. The ΔpH/ΔV should be on the vertical axis and the mean mL of NaOH should be on
the horizontal axis. Find the equivalence point by extrapolating peak position to
horizontal axis.
3. Use the relationship: N1V1 = N2V2 to determine the molarity of the monobasic acid
and therefore calculate the strength (Normality x equivalent weight) of the given
monobasic acid.
Given- Equivalent weight of the given monobasic acid = 60.05

WRITTEN BY: DR. ANIL MARKANDEYA and DR. NARAYAN FIRKE

2
 Linear Graph
Concentration Absorbance Absorbance Vs Concentration
1.0 0.70 1.00
0.9 0.61 y = 0.6727x + 0.0036
0.80
0.8 0.54 R² = 0.9964

Absorbance
0.7 0.46 0.60
0.6 0.39 0.40
0.5 0.32
0.4 0.28 0.20
0.3 0.21 0.00
0.2 0.15 -0.1 0.1 0.3 0.5 0.7 0.9 1.1
0.1 0.08 Concentration
0.0 0.00
Logarithmic Graph
[H+] pH pH Vs H+ Ion Concentration
0.026 1.58 1.70
0.030 1.52
y = -0.434ln(x) - 1E-14
0.040 1.40 1.50
R² = 1
0.045 1.35
pH

1.30
0.051 1.29
0.060 1.22 1.10
0.077 1.11
0.90
0.084 1.08 0.020 0.030 0.040 0.050 0.060 0.070 0.080 0.090 0.100
0.085 1.07
[H+]
0.093 1.03
Exponential Graph
Temprature Pressure
0 0.458
5 0.654 7 Temperature Vs Atmospheric Pressure
10 0.921
14 1.192
15 1.278
16 1.362 6
y = 0.5044e0.061x
17 1.452 R² = 0.9978
18 1.546
19 1.646 5
20 1.751
21 1.862
22 1.979
23 2.102 4
Temprature

24 2.232
25 2.369
26 2.513 3
27 2.665
28 2.825
29 2.994
30 3.171 2
31 3.357
32 3.57
33 3.759 1
34 3.975
35 4.202
36 4.44
37 4.69 0
38 4.951 0 5 10 15 20 25 30 35 40
39 5.226 Atmospheric Pressure
40 5.513